Materials Science & Engineering A 746 (2019) 332–340

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Tailoring mechanical behavior of a fine-grained metastable austenitic T

stainless steel by pre-straining
⁎
Chengsi Zhenga,b, , Heng Jianga, Xiyun Haoa, Juan Yea, Longfei Lic, Dehui Lid
a
National Safety Engineering Technology Research Center for Pressure Vessels and Pipelines, Hefei General Machinery Research Institute Co. Ltd., Hefei 230031, China
b
Hefei General Machinery Research Institute Special Equipment Inspection Station Co. Ltd., Hefei 230031, China
c
State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing 100083, China
d
Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201203, China

A R T I C LE I N FO A B S T R A C T

Keywords: A fine-grained AISI 304 austenitic stainless steel (ASS) was fabricated by cryogenic-rolling and cycle annealing.
Metastable austenite The fine-grained ASS was pre-strained to various strains of 0–0.16, and the corresponding microstructures,
Grain-refinement kinetics of strain-induced α′-martensite (SIMα′) and work-hardening behavior were investigated based on
Pre-strain quantitative characterization, interrupted-tensile tests and physical metallurgy. We find that the yield strength of
Kinetics
the ASS can be enhanced by combining grain-refining with pre-straining due to the strengthening effect of grain-
Mechanical behavior
refinement, dislocations, shear bands and SIMα′. The formation rate of shear band increases with increasing pre-
strain (εp) and the probability for an intersection of shear band to form a SIMα′ embryo is insensitive to the pre-
strain, and as a result, the kinetics of SIMα′ is accelerated by pre-straining. The fine-grained ASS with εp ≈ 0–0.16
display a three-stage work-hardening behavior, and the corresponding Stage I, II and III are completed in ad-
vance mainly due to their faster kinetics of SIMα′ and severer dynamic recovery caused by pre-straining. The
work-hardening rate (Θ) of pre-strained fine-grained ASS decreases faster than that of non-pre-strained coun-
terpart at Stage I, accompanying with dislocations-dominated hardening. The Θ ascend with increasing strain to
a peak value at Stage II and then decline continuously to necking at Stage III, following as SIMα′-governed
hardening, which can be tailored by grain-refining and pre-straining. Our studies provide the direct experimental
evidence for the pre-straining to trim the kinetics of SIMα′ in a fine-grained ASS. These observations help to
deepen understanding of the effect of pre-strain on the mechanical behavior of other fine-grained strengthening
ASS and transformation-induced-plasticity (TRIP) assisted alloy.

1. Introduction
Austenitic stainless steels are widely applied in industrial fields
because of their extraordinary combination properties of corrosion re-
sistance, mechanical properties, malleability and weldability [1–3]. The
intrinsic low yield strength of approximately 100 MPa [4] is a major
stumbling block to achieve the lightweight of ASSs equipment. To date,
there are two main approach to enhance the yield strength of ASSs, i.e.,
pre-straining and grain-refining [5,6]. The essence of reinforcement
resulting from pre-straining are the crystal-defects strengthening pro-
duced by lower strain and the SIMα′ strengthening caused by higher
strain [5,7]. The grain-refining to reinforce the yield strength and the
toughness is based on the universality Hall-Petch effect [8] in the field
of metallic materials. In particular, the dislocations density within ul-
trafine-grained ASSs (0.1–2 µm) can be effectively stored by the
formation of SIMα′ and strain-induced twin (SIT) [9,10], leading to that
the ultrafine-grained ASSs can maintain outstanding ductility and work-
hardening capability, which distinguish from the single-phase ultrafine-
grained ferritic steel and aluminum alloys [11,12], etc. Hence, the
grain-refining is a feasible method to simultaneously enhance the yield
strength and the toughness for ASSs without apparent reduction in
ductility and work-hardening capability. The ultrafine- or fine-grained
ASSs is usually prepared by using severe plastic deformation (SPD) to
transform single-phase coarse-grained austenite (γ) into deformed du-
plex (SIMα′ + γ) structure and subsequently annealing to reverse
transform into ultrafine- or fine-grained structure [6,13,14]. The ex-
perimental results of Kisko et al. [15] exhibit that there are a number of
dislocations to remain in austenite grains for an ultrafine- or fine-
grained ASS fabricated by cold-rolling and various annealing processes.
The pre-existing dislocations in ultrafine- or fine-grained ASSs will be

⁎
Corresponding author at: National Safety Engineering Technology Research Center for Pressure Vessels and Pipelines, Hefei General Machinery Research Institute
Co. Ltd., Hefei 230031, China.
E-mail address: zhengchengsi@126.com (C. Zheng).

https://doi.org/10.1016/j.msea.2019.01.038
Received 27 November 2018; Received in revised form 7 January 2019; Accepted 9 January 2019
Available online 11 January 2019
0921-5093/ © 2019 Elsevier B.V. All rights reserved.
C. Zheng et al.
further accumulated during the engineering-equipment manufacturing
due to unavoidable cold-working. Hence, it is necessary to discuss the
mechanical behavior of fine-grained strengthening ASSs after pre-
straining for their practical application.
The root of the enhancement in yield strength of an alloy by com-
bining grain-refining with pre-straining is to decrease the geometric slip
distance [16]. The mechanical behavior after yielding is strongly de-
pendent on the mechanical stability of austenite (MSA) which sig-
nificantly impacts on the work-hardening behavior via the kinetics of
SIMα′ for metastable ASSs [17]. There are experimental results
[10,18,19] to show that the MSA is obviously related to its grain size
and dislocations density, etc. The effect of grain size on the MSA has
been characterized quantitatively by using the increase in elastic strain
energy required for the transformation of face-centered cubic (f.c.c.)
austenite to body-centered cubic (b.c.c.) α′-martensite (ΔEV) [20]. The
ΔEV increases with decreasing average grain size of metastable ASSs,
accompanying with the suppression of the transformation of austenite
to SIMα′, especially when the grain size is refined to a comparable size
to martensitic lath [10,19]. Spencer et al. [21] have proved that the pre-
existing crystal-defects are incline to form stacking fault (SF) rapidly for
a coarse-grained ASS during tensile straining. Moreover, the intersec-
tions of SF are effective sites for the nucleation of SIMα′ [17], and
namely the kinetics of SIMα′ is accelerated for the coarse-grained ASS by
the pre-existing crystal-defects. In brief, it can be inferred that the ef-
fects of grain-refining and pre-existing crystal-defects on the formation
of SIMα′ are opposite, i.e., inhibition and promotion, respectively.
Hence, it is feasible to match average grain size and pre-existing crystal-
defects for enhancing the yield strength and maintaining a higher
uniform strain of metastable ASSs due to Hall-Petch effect [8], crystal-
defects strengthening and TRIP effect [22]. Specifically, the average
grain size of ASSs can be trimmed by various processes combining SPD
and annealing [23], and the pre-existing crystal-defects density can be
regulated by heat treatment and pre-straining.
Recently, there are plenty of experimental results to show that a
better strength-ductility synergy can be achieved by constructing an
ultrafine-grained ASS in comparison with coarse-grained counterpart,
and the corresponding macro- and micro-mechanical behavior are
elucidated in detail [10,19,24]. The strain-strengthening is commonly
applied to the coarse-grained ASSs [5,25,26] and has been put into
engineering practice of pressure equipment, and the performance be-
havior in the service environment is also discussed for the pre-strained
coarse-grained ASSs [27,28]. However, there are few works on the
mechanical behavior of pre-strained fine-grained ASS that can be rea-
lized in industry relatively easily, which is necessary to the application
of fine-grained ASS in the engineering-equipment. In this paper, an AISI
304 ASS is selected to fabricate a nearly single-phase fine-grained
structure by using cryogenic-rolling and cycle annealing, and the
crystal-defects density of the fine-grained ASS is further tailored by
using pre-straining. Moreover, the mechanical properties, work-hard-
ening behavior and SIMα′ kinetics of the fine-grained AISI 304 ASS with
pre-strain are discussed in comparison with that coarse- and fine-
grained counterpart without pre-strain for exploring the effect of grain-
refinement and pre-strain on mechanical behavior, which should be
easily extended to other metastable ASSs. The results are not only
beneficial to the design of equipment by using fine-grained strength-
ening ASSs but also the elucidation of mechanical behavior for pre-
strained TRIP-assisted alloy [29–31].
2. Experimental
The material studied was a commercial AISI 304 ASS with a che-
mical composition of 0.045 C, 1.11 Mn, 18.13 Cr, 8.25 Ni, 0.44 Si,
0.053 N, 0.0076 S and 0.034 P (mass%). The ASS was solution-treated
at 1100 °C for 30 min and then cut into a rectangular plate with a di-
mension of 150 × 40 × 8 mm3. The rectangular or deformed plate was
placed in liquid nitrogen for 20 min to ensure the plate temperature at
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Materials Science & Engineering A 746 (2019) 332–340
approximately −196 °C before each pass rolling, and then the plate was
cryogenic-rolled from 8 mm to 6.6 mm by multi-pass unidirectional
rolling, i.e., total true stain of approximately 0.19. Subsequently, the
deformed plate was annealed at 800 °C for 10 min with 1 cycle and
5 min with 2 cycles to fabricate a fine-grained structure mainly con-
sisting of single-phase austenite.
The microstructure observations were performed by using a scan-
ning electron microscope (SEM) and electron backscattered diffraction
(EBSD) in a Zeiss SUPRA55 field-emission SEM with a detector of
backscattered electrons and an orientation-imaging microscope (OIM).
The SEM and EBSD images were obtained to parallel the direction of
rolling [5]. The specimens were etched to reveal the α′-martensite
phase by using the standard method with two solutions in 1:1 ratio, i.e.,
0.20 g sodium-metabisulfate in 100 ml distilled water and 10 ml hy-
drochloric acid in 100 ml distilled water [32]. The α′-martensite phase
was showed as dark grey in the SEM image after etching 3 min. Spe-
cimens for EBSD analysis were electropolished by using an electrolyte
of 20% HClO4 + 10% glycerol + 70% C2H5OH under 15 V at room
temperature. The average grain size and the distribution of grain sizes
were measured from the EBSD images by using linear intercept method.
Thin foils for transmission electron microscopy (TEM, FEI Tecnai G2
F20 S-Twin, operated at 200 kV) were prepared by a precision ion
polishing system (Model 691, Gatan, Inc.), and the TEM images were
carried out to parallel the rolling or tensile direction. The chemical
compositions of austenite and α′-martensite were determined by en-
ergy-dispersive spectroscopy (EDS) in the TEM. The XRD measurement
was performed on SmartLab® diffractometer (Rigaku Corporation). The
amount of ferromagnetic α′-martensite (F) was evaluated by using a
Feritscope® (Helmut Fischer GmbH, model MP3E-S) based on ferro-
magnetism of α′-martensite. Feritscope testing were carried out in the
gage section to estimate the content of α′-martensite before and after
tensile testing, and the Feritscope was calibrated with standard samples
before measurement. The volume fraction of α′-martensite (Vα′) can be
converted by F and a coefficient of 1.42 [33], i.e., Vα′ = 1.42 F.
Tensile specimens were cut from the cryogenic-rolled and cycle-
annealed plate with a gage section of 25 × 6 × 1.4 mm3 [33], and the
tensile axis of specimens were machined along the rolling direction. The
surfaces of tensile specimens were mechanically polished sequentially
using wet sandpapers of 120–1000 grit at room temperature. The ten-
sile specimens were stretched to εp ≈ 0.073 and 0.16, respectively, by
using a custom built mechanical test system at a strain rate of 6 × 10−4
s−1 under room temperature. Subsequently, the tensile tests and in-
terrupted-tensile tests of the specimens with εp = 0, εp ≈ 0.073 and
0.16 were also conducted by using the mechanical test system at the
strain rate of 6 × 10−4 s−1 under room temperature. In addition, a
contact extensometer was used to measure strain in the gage of speci-
mens during all the pre-strain tests, tensile tests and interrupted-tensile
tests.
3. Results
3.1. Microstructure
The solution-treated AISI 304 ASS plate was cryogenic-rolled to a
total true strain of approximately 0.19 and the austenite grains were
transformed into the duplex (SIMα′ + γ) structure, which was further
verified by using SEM and XRD analysis (Vα′ ≈ 84%, Fig. 1) [33].
Fig. 2a shows the EBSD microstructure for the fine-grained ASS pre-
pared by the cryogenic-rolling and cycle annealing, exhibiting a mis-
chcrystal structure with an average size of austenite grains Dγ
≈ 5.2 ± 3.5 µm, and the corresponding size distribution of austenite
grains is shown in Fig. 2b. The Feritscope testing and EBSD observation
further reveal that the fine-grained ASS displays a practically single-
phase austenite structure with an initial volume fraction of recovered
SIMα′ (indicated by grey in Fig. 2a) V α0′ ≈ 1.9%. The selected area
electron diffraction (SAED) of Zone 1 and 2 in Fig. 3a correspond to
C. Zheng et al. Materials Science & Engineering A 746 (2019) 332–340

recovered SIMα′ and austenite, respectively, as shown in Fig. 3b and c.

The compositions analysis in Fig. 3d and e indicate that the recovered
SIMα′ contains less Ni, the former of austenite, than that of the auste-
nite. Hence, the micro-heterogeneity of chemical compositions may be
a reason for the unreversed SIMα′ to demonstrate more thermal-stability
than that of the SIMα′ to reverse into austenite in the fine-grained ASS.
Fig. 4a and b show a number of dislocations (indicated by arrows in
Fig. 4a) within austenite grains of the fine-grained ASS, which is similar
to the result of Kisko et al. [15]. The TEM observations of the fine-
grained ASS with εp ≈ 0.073 reveal that its tensile-microstructure
contains lots of dislocations and shear bands (indicated by arrows in
Fig. 4c and d). Additionally, the volume fraction of SIMα′ caused by pre-
straining (Vαp′) is approximately 7.2% in the fine-grained ASS with εp
≈ 0.073, and the Vαp′ is further up to approximately 30.6% when the εp
is increased to 0.16, which are increased by approximately 5% and 29%
in comparison with the state without pre-straining, respectively.

3.2. Mechanical properties

Fig. 1. SEM image (a) and XRD pattern (b) of the coarse-grained ASS after
cryogenic-rolling.
Fig. 2. EBSD image (a) and size distribution of austenite grains (b) for the fine-
grained ASS prepared by cryogenic-rolling and cycle annealing.
Fig. 5 shows the engineering stress-strain curves and the true stress-
strain curves of the fine-grained ASS with εp ≈ 0–0.16, and the corre-
sponding microstructural parameters and mechanical properties are
summarized in Table 1. The coarse-grained counterpart prepared by
solution-treatment is also displayed in Fig. 5 and Table 1 for compar-
ison. The yield strength (σy) of the fine-grained ASS is higher than that
of the coarse-grained ASS, i.e., 355 MPa vs. 248 MPa; however, its
tensile strength (σu) and uniform strain (εu) are less than that of coarse-
grained ASS, i.e., 1198 MPa vs. 1309 MPa and 0.36 vs. 0.48, respec-
tively. Moreover, the yield strength of fine-grained ASS is increased
from 355 MPa to 465 MPa by pre-straining to εp ≈ 0.073, and the
corresponding tensile strength and the uniform strain are decreased
slightly, i.e., 1198 MPa vs. 1109 MPa and 0.36 vs. 0.29, respectively.
When the pre-strain is increased from ≈ 0.073 to ≈ 0.16, the yield
strength and the tensile strength are further enhanced from 465 MPa to
638 MPa and 1109 MPa to 1176MPa, respectively, and the corre-
sponding uniform strain is decreased slightly from 0.29 to 0.21. Ad-
ditionally, the yield strength of fine-grained ASS with εp ≈ 0.16 is ap-
proximately 2.6 times higher than that of coarse-grained counterpart,
i.e., 638 MPa vs. 248 MPa. Generally, the yield strength of fine-grained
ASS can be enhanced significantly by pre-straining to a suitable εp (e.g.,
εp ≈ 0.073, 0.16) at the expense of a slightly decline in uniform strain,
exhibiting a better strength-ductility synergy in integrated view.
However, the strengthening effect of pre-strain on the tensile strength
can be neglected for the fine-grained ASS with εp ≈ 0–0.16. It can
further infer that the yield strength can be evidently enhanced by
combining grain-refining with pre-straining without the dramatic de-
cline of tensile strength and ductility for the ASS, which is a double-
strengthening pathway to achieve the lightweight of equipment which
designs based on the yield strength of ASS. To halve the weight of
current ASS equipment, the yield strength of fine-grained ASS should be
provided with more than twice that of coarse-grained ASS, i.e., σy
≥ 500 MPa. Consequently, the εp should be ranged from 0.09 to 0.16
extrapolating from the data in Table 1, and the optimal εp magnitude
depends on the design requirements for elongation, etc.
It should be noted that the enhancement of yield strength by com-
bining grain-refinement with pre-strain can be mainly attributed to the
Hall-Petch effect, crystal-defects strengthening and second-phase
(SIMα′) strengthening [34], and the core of all these mechanisms is to
decrease the geometric slip distance [16] for metastable ASSs. Ad-
ditionally, the characters of tensile strength and uniform strain chan-
ging with grain size and pre-strain are related to the work-hardening
behavior [35], which mainly attributes to the initial microstructure and
the kinetics of SIMα′ [17]. The pre-strain leads to changing the single-
phase fine-grained ASS into a hard-phase-strengthened alloy (Table 1)
with a number of crystal-defects, which will affect the microstructure
evolution and the kinetics of SIMα′. The difference between the volume

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Fig. 3. TEM image (a), SAED (b, c) and EDS (d, e) pattern of the fine-grained ASS prepared by cryogenic-rolling and cycle annealing.
fraction of SIMα′ at uniform strain (Vαs′) and V α0′ or Vαp′, i.e., ΔVα′, can be
deemed to as the total transformed Vα′ during uniform tensile straining,
and the ΔVα′/εu is a parameter to characterize the average growth rate
of SIMα′. The ΔVα′/εu of fine-grained ASS with εp ≈ 0.073 and 0.16 are
higher than that of non-pre-strained counterpart (Table 1), implying
that the pre-strain accelerates the kinetics of SIMα′ for the fine-grained
ASS, which will be discussed in detail in the next section.
4. Discussion
4.1. Effect of initial α′-martensite and pre-strain on the formation of SIMα′
4.1.1. Development of modified Olson-Cohen model
The Olson-Cohen model [17], a formula to establish a relationship
between the transformed fraction from austenite to SIMα′ (fα′) and
plastic strain (ε) based on physical metallurgy, is expressed as:
fα′ = 1 − exp(−βfsbn )
fsb = 1 − exp(−αε )
Materials Science & Engineering A 746 (2019) 332–340
( )(
fα′ = Vα′ − Vα′0 / 1−Vα′0 ) (1c)
where β and α are temperature-dependent constants during plastic de-
formation; n is a fixed exponent and is ≈ 4.5 for the ASS; fsb is the
volume fraction of shear bands (ε-martensite, mechanical twins and SF
bundles, etc.) in the austenite caused by plastic deformation. Specifi-
cally, the V α0′ is equal to 0 and Vαp′ for a non-pre-strained ASS without α′-
martensite and a pre-strained ASS, respectively.
According to Eqs. 1a-1c, the volume fraction of α′-martensite and
the volume fraction of shear bands in the non-pre-strained ASS with
initial α′-martensite, i.e., V′α′ and fsb ′ , are related to ε, which can be
expressed as:
( ) (
Vα′′ = 1− 1−V α0′ exp −bfsb
′ n1 ) (2a)
′ = 1 − exp(−aε )
fsb (2b)
where n1 is a fixed exponent for the non-pre-strained ASS with initial α′-
(1a) martensite; b and a are temperature-dependent constants during plastic
deformation.
(1b) In light of Eqs. (2a) and (2b), the volume fraction of α′-martensite
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Fig. 4. TEM images of the fine-grained ASS with and without pre-strain: (a, b) εp = 0; (c, d) εp ≈ 0.073.

and the volume fraction of shear bands in the pre-strained ASS, i.e., Vαp′ ( )
Vα′′′ = 1− 1−V α0′ exp { −[b [1 − exp(−aεp)]n1 + B [1 − exp(−Aε )]n2 ]}
and f sbp , are related to εp, which can be expressed as:
(6)
( ) (
Vαp′ = 1− 1−V α0′ exp −bf sbpn1 ) (3a) when there are not initial α′-martensite and pre-strain, i.e., V α0′ = 0 and
εp = 0, the Eq. (6) will be changed into the classical Olson-Cohen model
f sbp = 1 − exp(−aεp) (3b)
[17]. The Eqs. (5) and (6) are the modified Olson-Cohen model for the
Hence, the volume fraction of α′-martensite and the volume fraction non-pre-strained and pre-strained ASS with initial α′-martensite, re-
of shear bands in the pre-strained ASS during plastic deformation, i.e., spectively.
′ ′, are related to εp and ε, which can be obtained by combining
Vα′′′ and fsb
Eq. 1 with Eq. 3a:
4.1.2. Kinetics of SIMα′
( ) [ (
Vα′′′ = 1− 1−V α0′ exp − bf sbpn1 + Bfsb n
′′ 2 )] (4a) Fig. 6 shows statistical charts for the fα′ of the fine-grained ASS with
εp ≈ 0–0.16 and the coarse-grained ASS as a function of true strain (εt).
′ ′ = 1−exp(−Aε )
fsb (4b) The Olson-Cohen model (Eq. 1) is fitted to the data in Fig. 6 by using an
exponent of n = 4.5 and the corresponding model parameters are
where n2 is a fixed exponent for the pre-strained ASS with initial α′- summarized in Table 2. Obviously, the fα′ of the fine-grained ASS in-
martensite; B and A are temperature-dependent constants for the pre- creases with increasing εp at a same tensile strain, indicating that the
strained ASS during plastic deformation. MSA decreases with increasing density of crystal-defects caused by pre-
Combining Eq. (2a) and Eq. (2b), Vα′′ for the non-pre-strained ASS straining. The Vα′ of fine-grained ASS with εp ≈ 0–0.16 and coarse-
with initial α′-martensite can be rewritten as: grained ASS as a function of εt are plotted in Fig. 7, the α′-martensite
consisting of initial α′-martensite, SIMα′ caused by pre-straining and
( )
Vα′′ = 1− 1−V α0′ exp { −b [1 − exp(−aε )]n1 } (5)
SIMα′ generated during interrupted-tensile testing. The modified Olson-
when there is not initial α′-martensite, i.e., V α0′
= 0, the Eq. (5) will be Cohen model, Eq. (5), is fitted to the data of fine- and coarse-grained
changed into the classical Olson-Cohen model [17]. ASS in Fig. 7 by using an exponent of n1 = 4.5 and the corresponding
Combining Eq. (3b) and Eq. (4), Vα′′′ for the pre-strained ASS with model parameters are summarized in Table 2. The modified-model
initial α′-martensite can be rewritten as: parameters of a and b are similar to α and β of Olson-Cohen model for

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Fig. 6. Statistical charts for the transformed fraction from austenite to SIMα′ in
the fine-grained ASS with εp ≈ 0–0.16 and the coarse-grained ASS as a function
of true strain.

Fig. 5. Engineering stress-strain curves (a) and true stress-strain curves (b) of
the fine-grained ASS with εp ≈ 0–0.16 and the coarse-grained ASS. Note: FG and
CG refer to fine- and coarse-grained ASS, respectively, and the following are the
same.
the non-pre-strained fine-grained ASS, which attributes to the negli-
gible volume fraction of initial α′-martensite. The a, b and n1 of fine-
grained ASS are used as input parameters for the modified-model ap-
plicable to the pre-strained fine-grained ASS (Eq. (6)). The modified
Olson-Cohen model, Eq. (6), is fitted to the data of pre-strained fine-
grained ASS in Fig. 7 by using an exponent of n2 = 4.5 and the corre-
sponding model parameters are also summarized in Table 2. There are
numbers of works to state that the transformation of austenite to SIMα′
is suppressed by grain-refining, especially when the grain size is refined
to a comparable size to martensitic lath [10,15,19,24]. However, all of
fα′ in the fine-grained ASS with εp ≈ 0–0.16 are higher than that of
coarse-grained ASS at a same tensile strain, which implies that there
was another nonnegligible factor to affect the MSA besides the average
grain size [10]. In addition, the α of fine-grained ASS with εp ≈ 0–0.16
is higher than that of coarse-grained ASS and increases with increasing
εp for the fine-grained ASS. Nevertheless, the β is almost unchangeable
for the coarse-grained ASS and the fine-grained ASS with εp ≈ 0–0.16.
Moreover, the A also increases with increasing εp and the B is also in-
sensitive to pre-strain for the fine-grained ASS with εp ≈ 0–0.16. The α
and A represent the formation rate of shear band at low strains (Eq. 1b)
and increase with decreasing stacking fault energy (SFE) [17]. These
results indicate that the SFE of fine-grained ASS decreases with in-
creasing density of crystal-defects caused by pre-straining, which is
beneficial to the formation of SF. Furthermore, the pre-existing crystal-
defects are incline to form SF rapidly during tensile straining [21], and
this promotes the formation of SIMα′ since the intersections of SF are
effective sites for the nucleation of SIMα′ [17]. The β and B are pro-
portional to the probability for an intersection of shear band to form an
embryo and this probability is temperature dependent through its re-
lation to the chemical driving force [17]. Hence, the β and B of fine- and
coarse-grained ASS are insensitive to the crystal-defects density due to
the testing at room-temperature of ≈ 15 °C. Moreover, the A for the
pre-strained fine-grained ASS is slightly higher than the corresponding
α and the B for the pre-strained fine-grained ASS is similar to the
counterpart of β, which also indicates that the MSA decreases with
increasing density of crystal-defects caused by pre-straining. Summa-
rily, the pre-existing crystal-defects accelerate the kinetics of SIMα′
through decreasing the SFE, and as a result, the MSA decreases with
increasing density of crystal-defects caused by pre-straining. Hence, the
pre-existing crystal-defect is probably the nonnegligible factor to de-
crease the MSA of fine-grained ASS, which will be discussed in the
following.
4.2. Mechanical stability of austenite
The energy required for SIMα′ (ΔE) at room-temperature mainly
consists of the elastic strain energy for lattice displacement from f.c.c. to
b.c.c. structure (ΔEV) and the strain energy required for supplementary
deformation (ΔED) [10,36], i.e., ΔE = ΔEV + ΔED. In general, the lattice
displacement is made up of two atomic movements: shear deformation
of 36% to [1̅ 10] direction for supplementary deformation and aniso-
tropic deformation accompanying the volume expansion from f.c.c. to
b.c.c. structure [10,36].
The volume expansion consists of 13.9% expansion to [001] direc-
tion (I direction), 7.0% contraction to [1̅ 10] direction (II direction) and
1.4% contraction to [1̅ 1̅ 0] direction (III direction) [10,36]. The elastic

Table 1
Microstructural parameters and mechanical properties of the fine-grained ASS with εp ≈ 0–0.16 and the coarse-grained ASS.
Sample D (μm) V α0′ (%) εp Vαp′ (%) V αs′ (%) σy (MPa) σu (MPa) σy/σu εu ΔVα′/εu (%)

FG 5.2 ± 3.5 1.9 ± 0.2 / / 59.2 ± 0.8 355 1198 0.30 0.36 158.1
FG-0.073 5.2 ± 3.5 1.9 ± 0.2 0.073 7.2 ± 1.1 62.7 ± 1.1 465 1109 0.42 0.29 191.4
FG-0.16 5.2 ± 3.5 1.9 ± 0.2 0.16 30.6 ± 2.4 68.8 ± 2.8 638 1176 0.54 0.21 181.9
CG 48 ± 17 1.8 ± 0.2 / / 40.1 ± 1.1 248 1309 0.19 0.48 79.8

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Table 2
Model parameters for the fine-grained ASS with εp ≈ 0–0.16 and the coarse-grained ASS.
Sample α β n V0 (%) a b n1 εp A B n2

FG 9.4 0.94 4.5 1.9 ± 0.2 9.3 0.95 4.5 / / / /

FG-0.073 11.8 0.99 4.5 1.9 ± 0.2 9.3 0.95 4.5 0.073 12.2 0.99 4.5
FG-0.16 14.2 0.92 4.5 1.9 ± 0.2 9.3 0.95 4.5 0.16 16.5 0.90 4.5
CG 4.5 0.86 4.5 1.8 ± 0.2 4.6 0.83 4.5 / / / /

decrease in the MSA of a pre-strained ASS. Furthermore, the ΔE of fine-

grained ASS decreases with increasing the density of crystal-defects
caused by pre-straining, and the MSA of the fine-grained ASS decreases
with increasing pre-strain. It should be noted that the austenite in
coarse-grained ASS prepared by solution-treatment is more stability
than that of fine-grained ASS prepared by the cryogenic-rolling and
cycle annealing, i.e., ΔEFG < ΔECG, where ΔEFG and ΔECG are the ΔE of
fine- and coarse-grained ASS, respectively. According to ΔE = ΔEV
+ ΔED, the ΔEFG < ΔECG can be rewritten as:

∆E VFG−∆E VCG <∆EDCG−∆EDFG (10)

Fig. 7. Statistical charts for the volume fraction of α′-martensite in the fine-
grained ASS with εp ≈ 0–0.16 and the coarse-grained ASS as a function of true
strain.
where ∆E VFG and ∆E VCG are the ΔEV of fine- and coarse-grained ASS, i.e.,
≈ 24 MJ/m3 and 2 MJ/m3, respectively; ∆EDFG and ∆EDCG are the ΔED of
fine- and coarse-grained ASS, respectively. The results imply that the
promotion effect of pre-existing crystal-defects (Fig. 4) on SIMα′ is
higher than the inhibition effect of grain-refinement on SIMα′. In detail,
the difference in ΔED between coarse-grained ASS and fine-grained ASS
is higher than that in ΔEV between fine-grained ASS and coarse-grained
ASS (Eq. (10)).

strain energy for lattice displacement to accommodate over the space of

4.3. Work-hardening behavior
austenitic grain can be estimated as [10,36]:

∆EV = (1/2) EI εI2 (x / d )2 + [(1/2) EII εII2 + (1/2) EIII εIII2](x / d )
where EI = 132.1 GPa, EII = 220.8 GPa and EIII = 220.8 GPa are
Young's modulus in each lattice plane; εI = 0.139, εII = 0.07 and εIII
= 0.014 are elastic strain in each lattice plane; x is the thickness of
martensite plate, which is approximately of 0.2 µm [36]; d is the grain
size of austenite. The Eq. (7) can be rewritten as:
∆EV = 1276.1(x / d )2 +562.6(x / d )
According to Eq. (8), the transformation of austenite to SIMα′ is
suppressed by reducing grain size.
The supplementary deformation has to be introduced by dislocation
slip and twinning, etc. for accommodating the lattice displacement, and
the strain energy required for supplementary deformation can be esti-
mated as [36]:
∆ED = τω
where τ is shear stress of pure iron, which is approximately of
100–300 MPa [36]; ω is shear strain, which is approximately of 0.36
[36]; and the strain energy ΔED is approximately 36–108 MJ/m3.
Moreover, the ΔEV is much higher than the ΔED when the grain size is
refined to a comparable size to martensitic lath (d = 0.1–0.3 µm)
[10,19], i.e., 942–6230 MJ/m3 vs. 36–108 MJ/m3. Hence, the role of
ΔED can be ignored in comparison with the effect of ΔEV when the grain
size is approximately 0.3 µm.
The grain size of the fine- and coarse-grained ASS in this study are
approximately 5.2 µm and 48 µm, i.e., ΔEV ≈ 24 MJ/m3 and 2 MJ/m3,
respectively, and obviously the role of ΔED is indispensable in com-
parison with the effect of ΔEV. Additionally, when an ASS contains a
number of pre-existing crystal-defects, the lattice has been distorted and
the lattice displacement has been accommodated to some extent,
leading to the drop in the ΔEV caused by the decrease in overall elastic
lattice strain and the ΔED. In other words, the energy required for SIMα′,
ΔE, is declined due to the pre-existing crystal-defects, resulting in the
(7) Fig. 8a shows work-hardening rate Θ as a function of true strain εt
for the fine-grained ASS with εp ≈ 0–0.16 and the coarse-grained ASS.
The Θ-εt curves can be divided into three stages and the Θ-εt curve of
the fine-grained ASS is shown in the inset in Fig. 8a as an example.
Namely, the Θ decrease fast at Stage I and then ascend with the increase
of tensile strain to a peak value at Stage II, then following by a con-
tinuous decline to necking at Stage III. The end strain of Stage I, εI, the
(8) end strain of Stage II, εII, the interval strain of Stage II, ΔεII = εII - εI, and
the interval strain of Stage III, ΔεII = εu - εI are summarized for the fine-
grained ASS with εp ≈ 0–0.16 and the coarse-grained ASS in Table 3.
The εI, εII, ΔεII and ΔεIII of fine-grained ASS with εp ≈ 0–0.16 are lower
than that of coarse-grained ASS, and the counterparts of fine-grained
ASS decrease with increasing pre-strain, suggesting that the Stage I, II
and III are completed in advance by grain-refinement and pre-existing
crystal-defects (Fig. 4). It is evident that the rise rate of Θ in Stage II, the
drop rate of Θ in Stage I and III are all increased by pre-straining and
(9)
the peak value of Θ at Stage II (ΘII) grow with the increase of pre-strain.
The pre-existing α′-martensite and the pre-strain cause the single-
phase ASS to be a duplex (SIMα′ + γ) structure containing a number of
crystal-defects in the soft austenite matrix and the hard dispersed SIMα′.
Subsequently, the formation of SIMα′ further results in changing the ASS
into a duplex (SIMα′ + γ) ASS with continuous increase of SIMα′ and
crystal-defects during tensile straining. Hence, the work-hardening
behavior is probably related with the evolution of α′-martensite con-
tents and its increase rate for the fine-grained ASS with εp ≈ 0–0.16 and
the coarse-grained ASS. Fig. 8b and c show the curves of α′-martensite
contents Vα′ and its increase rate dVα′/dε vs. εt for the fine-grained ASS
with εp ≈ 0–0.16 and the coarse-grained ASS, respectively. Obviously,
although their Vα′ increase with increasing tensile strain, the dVα′/dε
grow with the increase of tensile strain to a peak value and then fol-
lowing by a continuous decline to necking, which both are different
with the three-stage characteristic of work-hardening. It is well-known
that the work-hardening behavior of an alloy is mainly governed by the
increase in crystal-defects to promote hardening and the dynamic

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geometric slip distance is decreased continuously by increasing the

interfaces density [29]. Moreover, although the hardening caused by
increasing SIMα′ is dominant, the dislocation slip and recovery in the
austenite gradually becomes more important at the later Stage II and
Stage III [29]. For the fine-grained ASS with εp ≈ 0, 0.073 and the
coarse-grained ASS, when the dVα′/dε decreases to a value, the corre-
sponding Θ start to decrease into Stage III. However, for the fine-
grained ASS with εp ≈ 0.16, the Θ begin to decrease into Stage III when
the dVα′/dε is still increasing, which implies that the dynamic recovery
of fine-grained ASS with εp ≈ 0.16 is more severe than that of other
counterparts during Stage II. This is probably related with its higher
volume fraction of initial SIMα′ (Vαp′ ≈ 30.6%) beside the high initial
dislocations density in the austenite matrix, since the dislocations
density cannot be stored effectively in the ultrafine-grained b.c.c.
structure [42]. In short, the faster kinetics of SIMα′ and the severer
dynamic recovery caused by pre-straining lead to the early start and
end of Stage II, respectively, for the pre-strained fine-grained ASS
(Fig. 8). Moreover, the severer dynamic recovery caused by pre-
straining also leads to the falling rate of Θ at Stage III to increase with
increasing pre-strain for the fine-grained ASS with εp ≈ 0–0.16.
In summary, the pre-strain results in the single-phase fine-grained
ASS to change into a duplex (SIMα′ + γ) fine-grained ASS containing a
number of crystal-defects. As a result, the corresponding kinetics of
SIMα′ was accelerated due to the decrease of SFE or ΔE, which was
embodied in the effect on work-hardening behavior. According to the
Considére criterion [43], σ ≤ Θ, where σ is the true stress, the work-
hardening behavior is the critical factor to affect the uniform strain for
a fine-grained strengthening ASS due to its higher yield strength. The
work-hardening behavior of the fine-grained strengthening ASS was
mainly affected by the kinetics of SIMα′ [9,20], which can be suppressed
by grain-refining and accelerated by pre-straining. Additionally, it can
Fig. 8. Work-hardening rate (a), α′-martensite content (b) and the increase rate
be inferred that not only the yield strength of the fine-grained
of SIMα′ (c) as a function of true strain for the fine-grained ASS with εp strengthening ASS will be further increased by using cold-work to
≈ 0–0.16 and the coarse-grained ASS. manufacture equipment, but also the corresponding SIMα′ will be
formed more quickly than that without cold-working when they are
plastic-deformed by the external force.
Table 3
The end strain of Stage I and II, the interval strain of Stage II and III, and the
peak value of Θ at Stage II for the fine-grained ASS with εp ≈ 0–0.16 and the
5. Conclusions
coarse-grained ASS.
A fine-grained AISI 304 ASS with εp ≈ 0–0.16 was selected to in-
Sample εI εII ΔεII ΔεIII ΘII (MPa)
vestigate the role of pre-strain in the mechanical behavior for me-
FG 0.070 0.22 0.15 0.14 2671 tastable alloy strengthened by grain-refining. The corresponding mi-
FG-0.073 0.018 0.13 0.11 0.16 2793 crostructures, mechanical properties, kinetics of SIMα′ and work-
FG-0.16 0.013 0.048 0.035 0.16 3460 hardening behavior were discussed based on quantitative character-
CG 0.10 0.32 0.22 0.16 2625
ization, interrupted-tensile tests and physical metallurgy. The main
results and conclusions are the following:
recovery to cause softening [37]. The growth ability of crystal-defects
1. The fine-grained ASS prepared by cryogenic-rolling and cycle an-
can be enhanced by the hard second-phase for an alloy containing soft
nealing contained a number of dislocations within austenite grains.
matrix [38,39], and hence the evolution of α′-martensite contents and
The pre-strained counterpart included dislocations, shear bands and
its increase rate play leading role in the growth ability of crystal-defects
SIMα′, resulting in that the yield strength of ASS was enhanced by
for the ASS. The rate of dynamic recovery has positive correlation to the
combining grain-refining with pre-straining.
crystal-defects density and becomes intense with the increase of tensile
2. The MSA of fine-grained ASS decreased with increasing crystal-de-
strain during work-hardening according to the Kocks-Mecking model
fects density caused by pre-straining, which was embodied in the
[40]. Additionally, the dynamic recovery can be further intensified due
accelerated kinetics of SIMα′.
to the temperature rise caused by plastic deformation during work-
3. The modified Olson-Cohen model demonstrated that the forming
hardening [41].
rate of shear band increased with increasing crystal-defects density
The microstructural evolution during Stage I is characterized by the
caused by pre-straining, and the probability for an intersection of
generation of dislocations in austenite matrix [10] and the increment of
shear band to form a SIMα′ embryo was insensitive to the pre-strain.
SIMα′ can be almost ignored for the fine-grained ASS with εp ≈ 0–0.16
4. A three-stage work-hardening behavior showed in the fine-grained
(Figs. 4a and 7b). The pre-existing dislocations cause more severe dy-
ASS with εp ≈ 0–0.16, and all the three stages were completed in
namic recovery [40] in the pre-strained fine-grained ASS, accom-
advance due to their accelerated kinetics of SIMα′ and enhanced
panying with a faster decrease in the Θ than that of non-pre-strained
dynamic recovery by pre-straining.
counterpart during Stage I. In Stage II, the formation of SIMα′ and
crystal-defects bring increasing obstacles of dislocation slip to cause
hardening through the dynamic Hall-Petch effect [8,29] that means the

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C. Zheng et al.
Acknowledgments
Financial support from the National Natural Science Foundation of
China (51601052) and from the Natural Science Foundation of Anhui
Province (1708085QE95) is gratefully acknowledged. We would like to
express our sincere thanks to Prof. Yandong Wang, Prof. Zuqing Sun
and Prof. Wangyue Yang from the University of Science and Technology
for discussing the effect of microstructure evolution on mechanical
behavior. We would also like to express our sincere thanks to Ph.D.
Defu Nie from the Hefei General Machinery Research Institute Co. Ltd.
for the help of TEM specimen preparation.
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